Integrated micro-solid-phase extraction with miniature mass spectrometry for on-site detection of illicit drugs in human hair.

Abstract

This study presents a novel, integrated micro-solid-phase extraction/miniature mass spectrometry (micro-SPE/mini-MS) platform designed for the rapid, on-site quantification of conventional illicit drugs and emerging new psychoactive substances (NPS) in human hair. The system addresses the critical need for laboratory-grade accuracy in field settings by coupling a streamlined, mixed-mode cation exchange (MCX) pipette-tip micro-SPE protocol with a miniaturized mass spectrometer utilizing paper-capillary spray (PCS) ionization. The method targets three conventional illicit drugs, methamphetamine (MA), 3,4-methylenedioxymethamphetamine (MDMA), and ketamine (KET), and three new NPS, etomidate (ETM), isopropoxate (IPX), and 2-oxo-PCE. By systematically optimizing the micro-SPE enrichment and mini-MS parameters, we achieved significant mitigation of matrix effects, yielding impressive limits of detection (LOD, 1-3 ng/mL in hair extract) and robust linearity (R² ≥ 0.9917). The entire analytical workflow, from sample preparation to result, is completed within 5 min, offering a drastic reduction in turnaround time compared to traditional chromatography-based methods. Validation using authentic hair samples previously confirmed by laboratory LC-MS/MS demonstrated superior quantitative consistency, with relative errors maintained within 15%. By bridging the gap between rigorous laboratory confirmation and point-of-need screening, this field-deployable platform represents a significant advancement in forensic toxicology, workplace drug testing, and clinical diagnostics.

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